CN1142719C

CN1142719C - Ice confection

Info

Publication number: CN1142719C
Application number: CNB008073864A
Authority: CN
Inventors: A; A·达尼尔; R·A·芬; ˹��ͼ˹��µ�; J·R·奥德罗伊德
Original assignee: Unilever NV
Current assignee: Unilever NV
Priority date: 1999-03-10
Filing date: 2000-03-02
Publication date: 2004-03-24
Anticipated expiration: 2020-03-02
Also published as: IL145155A0; IL145157A; EP1158863B1; US6436460B1; DK1158862T3; ATE279864T1; BR0008887A; AU765323B2; DE60034970D1; ES2228484T3; BR0008889A; IL145154A; CA2363241C; DE60014865T2; AU765718B2; DE60014865D1; CA2362725A1; DE60020339D1; US6503548B1; CN1129369C

Abstract

An unaerated ice confection in the form of thin, unsupported, discrete pieces which are stable during packaging, storage and distribution wherein the ice confection comprises an antifreeze protein and has the following mechanical properties; DELTA modulus/original modulus >/= 0.4, and/or DELTA strength/original strength >/= 0.4; providing that when DELTA modulus/original modulus </= 6.0, DELTA modulus >/= 50MPa, and/or when DELTA strength/original strength </= 2.0, DELTA strength >/= 0.2MPa.

Description

Ice confection

Technical field

The present invention relates to contain the new ice confection of antifreeze protein.The present invention relates to the new ice confection that the nothing that approaches supports the discrete patch form specifically, this ice confection is at packing, storage and be stable between allotment period.

Background of invention

People expect to make the ice confection with new shape, performance and/or quality very much.Yet, make product have the novelty of high level so far and the ability of interest is limited.Have to onlyly pack, storage and sales force manufactures a product.

Specifically, also cannot provide slim nothing to support the sheet ice confection so far, make it enough stably tolerate packing, storage and assigning process.In addition, also cannot provide thin nothing to support the sheet ice confection, it still be crisp, hard and crisp but still (that is, when inlet they can fragmentation) that can sting simultaneously.Obviously, this thin, crisp, crisp goods have king-sized cracked possibility between packing or delivery period.

We find to comprise specific antifreeze protein in the ice confection of unaerated now, can form continuous ice crystal net firm, that closely enrich in ice confection.As a result, make ice confection have the mechanical performance of certain well.This ice confection can be manufactured into thin no support chip, and it is crisp and crisp, but still can tolerate packing, storage and transportation.

WO 98/04146 (Unilever) discloses in the frozen food goods that AFPs can be spiked into such as ice confection, so that required properties of product to be provided, prerequisite is to change product and process conditions, so that the length-width ratio of the ice crystal that forms in product is greater than 1.9, preferred 1.9-3.0.Given specific embodiment is that the ice river in Henan Province of inflation is insulted composition fully.Shown in following Comparative Examples A-C, insult the interpolation antifreeze protein to inflation ice river in Henan Province and can not change the mechanical performance that the ice river in Henan Province is insulted significantly.WO 98/04146 does not have instruction can provide specific ice confection goods and this ice confection with new mechanical performance can advantageously be used to provide thin no support chip.

WO 96/39878 (The Pillsbury company) discloses a kind of production method of the frozen composition of being convenient to store, and this method did not need cure step before storage.This frozen composition contains antifreeze protein, is I type AFP specifically.Embodiment has shown that inflation ice river in Henan Province is insulted and the preparation of aerated frozen sour milk.Shown in following Comparative Examples A-C, insult the interpolation antifreeze protein to inflation ice river in Henan Province and can not change the mechanical performance that the ice river in Henan Province is insulted significantly.WO 96/39878 does not have instruction can provide specific ice confection goods and this ice confection with new mechanical performance can advantageously be used to provide thin no support chip.

US 5 118 792 (Warren etc.) discloses fusion albumen, is fusion albumin A-Saf5 specifically, add in the frozen food that can eat, for example, ice river in Henan Province icepro, fro-yo, ice milk, ice cream, ice lolly and freezing whipping rare cream that bubbles.Not having embodiment to provide wherein finished product ice confection contains this fusion albumen and provides.Embodiment 3B shows that the growth of ice crystal is restricted when using the ice lolly prescription in " the Quench sheet is measured (splat assay) ".

Our not examining among the application PCT/EP98/085 52 (being disclosed in 1999.7.29 with WO 99/37164, after the application's priority date), a kind of frozen food goods are disclosed, the AFPs that it contains average ice crystal granularity is the 0.01-20 micron.This application is devoted to reduce as much as possible the gathering of ice crystal, so that soft, creaminess goods are provided.Embodiment discloses and has iced the manufacturing that river in Henan Province is insulted flat thin slice.Yet, used ice river in Henan Province insult be inflation and according to shown in following Comparative Examples A-C, this ice river in Henan Province is insulted flat thin slice and can not self be supported, so that they subside in storage and assigning process.But WO 99/37164 openly can not provide the ice confection of the thin discrete sheets of self supporting, it is at storage and to divide timing be stable, and ice confection has specific mechanical performance.

Disclosure of the Invention

Therefore, the invention provides the ice confection that a kind of thin nothing supports the unaerated of discrete patch form, it is at packing, storage and be stable between allotment period, and wherein ice confection contains antifreeze protein and has following mechanical performance:

Δ modulus/original modulus 〉=0.4, and/or

Δ intensity/green strength 〉=0.4; Precondition is to work as

△ modulus/original modulus≤6.0 o'clock, Δ modulus 〉=50MPa, and/or when Δ intensity/green strength≤2.0,

Δ intensity 〉=0.2MPa.

" approach " and mean 5mm or littler thickness.Typically, the thickness of thin layer is 0.5-5mm.Particularly about 2-3mm.

" sheet " mean for example flat thin slice, sheet, flat, tabular, chip, fragment, ring plate, crackling or layer.Usually, sheet is not spherical.All sizes are also inequality.A size is that 0.5-5mm and at least one other size are longer than this size basically.

" do not have support " means thin crispy pieces and only contacts with air basically, and is not, for example, is positioned at second kind of layer above the ice confection, and wherein said second kind of ice confection is the thin layer body that provides support.

Preferably, Δ modulus/original modulus 〉=0.4; Precondition is when Δ modulus/original modulus≤6.0, and Δ modulus 〉=70MPa is preferred 〉=90MPa, first-selection 〉=100MPa.

First-selection, Δ modulus/original modulus 〉=1.0; Precondition is when Δ modulus/original modulus≤6.0, and Δ modulus 〉=100MPa is preferred 〉=200MPa.

Preferably, Δ intensity/green strength 〉=0.7.First-selection, Δ intensity/green strength 〉=1.5.

" modulus " means the apparent elastic modulus (E) that uses four-point bending test to measure.Embodiment 1 will provide the standard method of carrying out four-point bending test.

Therefore, to mean aspect prescription and manufacturing process all identical, difference be to contain antifreeze protein during first kind of ice confection formed and do not contain modulus change between two kinds of ice confections of antifreeze protein (reference composition) in second kind of ice confection composition to Δ modulus (Δ E).Original modulus (E _Original) be the modulus of measuring in the reference composition.

" intensity " means bending strength (σ _u), it can be defined as the maximum stress that material under given conditions can tolerate.The power that writes down in four-point bending test is thought bending strength to the stress at the some place of the maximum, force on the displacement curve.

Therefore, Δ intensity (Δ σ _u) to mean aspect prescription and manufacturing process all identical, difference be to contain antifreeze protein during first kind of ice confection formed and do not contain Strength Changes between two kinds of ice confections of antifreeze protein (reference composition) in second kind of ice confection composition.Green strength (σ _{U is original}) be the modulus of measuring in the reference composition.

The variation in apparent elastic modulus and bending strength, ice confection of the present invention can provide the increase of product hardness.

Concerning passing through the freezing ice confection of stirring, for example to insult in the refrigerator (as the scraper-type heat exchanger) at the ice river in Henan Province, the increase of hardness can use Wei Keersi hardness (Vickers hardness) test to measure.The content of Wei Keersi hardness test is seen embodiment 3.

Add antifreeze protein and increase ice confection Wei Keersi hardness (H _V) degree depend in part on ice content in the ice confection.

Yet, as a rule, Δ H _V/ H _{V is original}〉=0.3, precondition is as Δ H _V/ H _{V is original}≤ 5.0 o'clock, Δ H _V〉=0.3.

Preferably, Δ H _V/ H _{V is original}〉=1.0, precondition is as △ H _V/ H _{V is original}≤ 5.0 o'clock, Δ H _V〉=1.25.

First-selection, Δ H _V/ H _{V is original}〉=6.0, perhaps Δ H _V/ H _{V is original}≤ .60 and Δ H _V〉=2.0.

Δ H wherein _VMean aspect prescription and manufacturing process all identical, difference and be and contain antifreeze protein during first kind of ice confection formed and do not contain Wei Keersi firmness change between two kinds of ice confections of antifreeze protein (reference composition) in second kind of ice confection composition.H _{V is original}Be the original Wei Keersi hardness of measuring in the reference composition.

The ice crystal that " the closely substantial continuous net of ice crystal " means any one appointment all is connected with at least one other ice crystal.

Can recently measure by contact by stirring in the freezing unaerated ice confection, net the degree that forms.Contact gear ratio is defined as particle and particle contact-making surface (interface) the area ratio divided by total contact-making surface (interface) area.The net of measuring the particle phase thus forms degree.Embodiment 4 has shown the assay method of contact gear ratio.

Unaerated ice confection of the present invention, when when measuring down for-18 ℃, concerning the ice content of 50-90wt%, preferred 54-85wt%, its contact gear ratio is at least 0.2.

In the unaerated ice confection freezing by any means, the degree that net forms can be measured by the Euler-Poincare index (Euler-Poincare characteristic) of ice phase.Euler-Poincare index is the measured value that the net of specific phase forms degree.The value of Euler-Poincare index is low more and negative more, big more at the continuity of phase.Embodiment 5 has shown the assay method of Euler-Poincare index.

Unaerated ice confection of the present invention, when when measuring down for-18 ℃, concerning the ice content of 50-90wt%, preferred 54-85wt%, the test determination that its ice phase Euler-Poincare index provides by embodiment 5 is for less than-150mm ^-2

" AFP " means has the obvious ice protein of crystallization inhibition again, and said ice crystallization inhibition is again measured according to embodiment 2.Ice pellets granularity when AFP provides less than the crystallization again of 20 μ m, more preferably 5-15 μ m.

Contain the antifreeze protein of 0.0005wt% at least in the preferred ice confection, more preferably the antifreeze protein of 0.0025wt%.Typically, the antifreeze protein that contains 0.0005wt%-0.005wt% in the ice confection.

Concerning some purposes, it is favourable that two or more different AFPs are included in the food article.

The AFP that is used for goods of the present invention can be the AFP that any suitable food article uses.The for example visible article " antifreeze protein and the potential use in frozen food thereof " of the example in the suitable source of AFP, Marylin Griffith and K.Vanya Ewart, " biotechnology progress " (Biotechnology Advances), the 13rd volume, the 375-402 page or leaf, 1995 and patent application WO 98/04699, WO 98/04146, WO 98/04147, WO 98/04148 and WO 98/22591.

AFPs can obtain from their source by any suitable method, for example the partition method of describing in the above-mentioned document of mentioning.

A kind of possible source of AFP material is a fish.The example of fish AFP material is antifreeze glycoprotein (AFGP) (for example, can obtain from Atlantic Ocean cod, Greenland cod and tomcod); I type AFP (for example, can obtain) from winter flounder, yellowtail flounder, shorthorn sculpins (Shorthorn sculpin) and living maggot sculpins (Grubby sculpin); II type AFP (for example, can obtain from America suede Du Wen fish, smelt and Atlantic Ocean catfish) and III type AFP (for example, can obtain from America macrozoarces americanus, Atlantic Ocean wolffish, luminous hilsa herring (Radiatedshanny), rock brocade Blenniidae (Rock gunnel) and draw Wo Shi silk floss cod (Laval ' s eelpout)).The preferred embodiment of latter's type is described in WO 97/02343 to some extent.

The source of the AFP material that another kind is possible is an invertebrate.AFPs can also obtain from bacterium.

The third source of AFP material is a plant.The example that contains the plant of AFPs is garlic-leaf mustard, blue wooden aster belongs to (blue wood aster), spring oats, winter Chinese celery, winter Canada's rapeseed (wintet canola), brussels sprout, carrot, Dutchman's-breeches, Euphorbia, day lily, winter barley, Virginia rolling chrysanthemum (waterleaf), the narrow leaf Asiatic plantain, Asiatic plantain, sword grass (speargrass), the Kentucky bluegrass, the east cottonwood, white oak, winter rye, bitter sweet Solanum (bittersweetnightshade), potato, chickweed, dandelion, spring wheat and winter wheat, triticale, catharanthus roseus, Viola and grass.

Can use naturally occurring kind, also can use the kind that obtains by genetic modification.For example, microorganism or plant are carried out genetic modification to express AFP, be used for the present invention then.

Can use gene manipulation techniques to produce AFPs.Can use gene manipulation techniques to produce to have at least 80% with the AFPs that from the plant source of the natural AFPs of containing, directly obtains, more preferably more than 95%, the AFPs of first-selected 100% homology.For purposes of the present invention, these AFPs with high-level homology also belong to the scope of term " AFP ".

Gene manipulation techniques can followingly use: transform suitable host cells or biology by the gene construct that comprises required polypeptide.The nucleotide sequence that is used for coded polypeptide can be inserted suitable expression vector, wherein said vector encoded is used to the unit of necessity of transcribing and translating, and with they under optimum conditions (for example, with the frame of suitable orientation and correction and have suitable target-seeking and the expressed sequence) mode that can be expressed carry out.The method that making up these expression vectors needs is known for a person skilled in the art.

A lot of expression systems all can be used for the express polypeptide coded sequence.Comprising (but being not limited thereto) bacterium, yeast, insect cell system, culture plant cell system with all with suitable expression vector plant transformed.

Can transform various plants and plant cell system with the constructs of required polypeptide.Embodiment preferred comprises (but being not restricted to this) corn, tomato, tobacco, carrot, strawberry, rapeseed and beet.

Concerning some natural origins, AFPs may be made up of the mixture of two or more different AFPs.

Select preferred antifreeze protein so that it to make ice crystal reach length-width ratio greater than 1.9, preferred 1.9-3.0, more preferably 2.0-2.9, more preferably 2.1-2.8 (referring to WO 98/04146).

Length-width ratio is defined as the maximum gauge of particle divided by its minimum diameter.Length-width ratio can be measured by any suitable method.Embodiment has introduced a kind of preferable methods in (embodiment 6).

For purposes of the present invention, preferably AFPs is obtained from fish.Especially preferably use III type fish albumen, the HPLC 12 that describes among our the application WO 97/02343 of first-selection.

What can form that ice confection that thin nothing supports discrete patch and can show the required variation of mechanical performance because added antifreeze protein comprises unaerated contains the milk frozen confection, as ice river in Henan Province icepro, frozen yogurt and freeze egg milk, sherbet (sherbet) and milk ice and the typical frozen confection that does not contain the unaerated of milk, as the syrup ice cream, with frozen water (sorbet), the granita of fruit wine or fruit juice with freeze puree.

Preferably, ice confection is selected from the ice river in Henan Province of unaerated and insults, syrup cake ice and milk ice.

" syrup ice cream " means the frozen soln of being made by sugar, water, tartaric acid or other acidulant, colouring agent, fruit or fruit flavor agent basically.

" unaerated " means swell increment is 10% or the ice confection of littler (being equivalent to 0.09 parts by volume air).In the process of ice confection, do not consider the step of bubbling product gas content is increased such as beating.Yet, will be appreciated that in the normal method of preparation unaerated ice confection, have a small amount of gas or air and sneak in the product, for example owing to used mixing condition.

Preferably, be used for providing unaerated ice confection thin, no support chip, ice content is when typically being at least 30% volume when measuring down for-18 ℃, more preferably when be at least 40% volume when measuring down for-18 ℃, first-selected when be at least 50% volume when measuring down for-18 ℃.

Ice content can be measured in the technology described in the article of " food engineering magazine " (Journal of Food Engineering) the 24th volume 405-415 page or leaf (1995) according to B de Cindio and S Correra.Use heat-insulating calorimetry (Holometrix adiabatic calorimeter) to obtain the needed enthalpy data of this technology.Herein, expressed ice content is measured the 80g sample, wherein said sample first impouring calorimeter sample before putting into calorimeter (being chilled to-70 ℃ to-80 ℃ in advance) stores device and assembly is put into dry ice and is cooled to-75 ℃, method according to Cindio and Carrera, analyze the enthalpy data that obtained and obtain ice content, it is the function of temperature.

Preferably, at the unaerated ice confection that is used for providing no support slice, total dissoluble solid content is less than 40wt%, and is preferably less than 25wt%, first-selected less than 15wt%.Concerning lower calories prod, total dissoluble solid content for example can be low to moderate approximately 5wt%.

Total dissoluble solid content is at the wt% that measures and be total composition dissolved under this temperature under 4 ℃.

The present invention does not have support slice, and the tendency of its gathering is reduced, thereby can keep the free mobility of particulate matter at storage period, even like this when storage temperature is high relatively yet.

The present invention is particularly suitable for making the frozen confectionery products that is similar to local delicacies, crackling for example, ring plate, thin crisp short cakes with sesame, thin rod etc.Typically, various snack based articles have the volume of 0.5-40ml, more preferably 1-20ml, particularly 1.5-10ml.

Another example of the present invention is flat lollipop.

Thin no support chip can provide by any suitable method.

First illustrative methods of the no support slice of manufacturing comprises the ice confection film of unaerated static freezing on the drum-type refrigerator of slowly rotation, scrapes frozen coating then.The frozen coating fragmentation is obtained discrete flat laminar.

Second illustrative methods making no support slice is by extruding.

Accompanying drawing describes in detail

Fig. 1 has shown the schematic diagram of record data during or the four-point bending test at 3.

Fig. 2 has shown that exemplary force is to the schematic diagram of displacement curve in the Wei Keersi hardness test.

In Fig. 3-13, contain the embodiment of AFP by () expression, do not contain the control sample of AFP by (◆) expression.

Fig. 3 has shown the apparent modulus of embodiment 9-12 mensuration and the comparison of control sample.

Fig. 4 has shown the bending strength of embodiment 9-12 mensuration and the comparison of control sample.

Fig. 5 has shown the Wei Keersi hardness of embodiment 9-12 mensuration and the comparison of control sample.

Fig. 6 has shown the comparison of apparent modulus with Comparative Examples A, B and C and the relevant control sample of embodiment 13 mensuration.

Fig. 7 has shown the bending strength of embodiment 13 mensuration and the comparison of Comparative Examples A, B and C and relevant control sample.

Fig. 8 has shown the Wei Keersi hardness of embodiment 13 mensuration and the comparison of Comparative Examples A, B and C and relevant control sample.

Fig. 9 has shown the apparent modulus of embodiment 14-17 mensuration and the comparison of control sample.

Figure 10 has shown the bending strength of embodiment 14-17 mensuration and the comparison of control sample.

Figure 11 has shown the Wei Keersi hardness of embodiment 14-17 mensuration and the comparison of control sample.

Figure 12 has shown the apparent modulus of embodiment 18-21 mensuration and the comparison of control sample.

Figure 13 has shown the bending strength of embodiment 18-21 mensuration and the comparison of comparative sample.

Embodiment

The present invention will illustrate by the mode of following examples.

Embodiment 1

Four-point bending test

Use standard four-point bending test can be measured many mechanical performances of ice confection material.

The mechanical performance of measuring is Young's modulus (apparent) and bending strength.

In bend test, make test block distortion, measure the power that applies and the deflection of test block simultaneously.The n-lustrative data group of ice confection is shown among Fig. 1.The slope (gradient) that begins straight line portion according to this curve is measured apparent elastic modulus.

4-point bend test need be produced the parallel edges sq.rd of ice confection material.This can obtain by any suitable means.

In this specific application, use aluminum die to make the parallel edges sq.rd of ice confection, produce the rod that is of a size of 25 * 25 * 200mm.

A) static freezing ice confection

In liquid ice confection pre-composition impouring mould,, then mould is put into-35 ℃ airflow freezing machine at least 2 hours with said mould in-35 ℃ airflow freezing machine pre-cooled at least 30 minutes.Store until test (carrying out after 5-6 days) down with the sample demoulding and at-25 ℃ then.Preceding 18-24 hour of test makes its balance with sample by storing down at-18 ℃, and-18 ℃ is the temperature of carrying out Total Test.Every sample sets is tested minimum 10 rods, and the mean value that writes down each sample sets is as tested mechanical behavior value.

B) stir freezing ice confection

Ice confection is expressed in the mould pre-cooled 30 minutes in-35 ℃ of downstream refrigerators from-1 ℃ to-5 ℃ ice river in Henan Province icepro refrigerator (scraper-type heat exchanger) at least, the temperature of wherein icing river in Henan Province icepro refrigerator depends on ice confection, and mould uses the silicon paper substrates in case stagnant ice-metlbond.Then, the mode by above-mentioned static freezing sample prepares sample.

The general test that is fit to all types solid is described in " biomethanics material; a kind of hands-on approach (Biomechanics Materials.A practical Approach) " J.F.V.Vincent and compiles, IRL Press publishes, the Oxford University Press, Walton Street, the Oxford, 1992 and " plastics testing material handbook (Handbook of Plastics Testmaterials) " R.P.Brown compile, George Godwin Limited publishes, TheBuilder Group, 1-3 Pemberton Row, Fleet Street, London, 1981.Test comprises each club is placed on 2 carriers, and makes it crooked, and the carrier central authorities that make the club upper surface that exert pressure produce fracture (carrier is at a distance of 85mm above said two) above by two.Crooked applied force of record and the mobile displacement that contacts in entire test.The decrease speed of mobile vehicle is per minute 50mm.

Provide the apparent elastic modulus of material by following equation:

Wherein slope is shown in Figure 1, and S is the span (distance) between the carrier below the prod contacts, and B is the width of club and the degree of depth that D is club.

In these tests, span (S) is 170mm.

With reference to figure 1, the intensity of material under three-point-bending conditions is

σ wherein _uBe bending strength and F _MaximumIt is the maximum, force of record.

Embodiment 2

Whether AFP has is iced the assay method of crystallization inhibition again

The crystallization inhibition can use improvement " the Quench sheet is measured (splatassay) " (Knight etc., 1988) to measure again.30% (w/w) sucrose solution that 2.5 μ l need be tested moves on the circular slide cover (coverslip) of a 16mm clean, suitably mark.With second slide cover be placed on drips of solution above, and this sandwich is pressed on together with forefinger and thumb.This sandwich input is arranged in-80 ℃ the hexane bath of remaining on of dry ice box.When having prepared all sandwich, use the pliers of precooling in dry ice, sandwich is transferred in the observation ward that maintenance-6 ℃ hexane is housed from-80 ℃ of hexane bath.When being transferred to after-6 ℃, the outward appearance that can see sandwich from transparent become opaque.By the video cameras recording picture and grab ias (LUCIA, Nikon) in, use 20x object lens (objective).O'clock write down the image of each Quench sheet (splat) in time=0, and after 60 minutes recording picture again.With slide glass be put into controlled temperature cryostat (Bright Instrument Co., Ltd, Huntington, UK) in, the size of the ice crystal in two analyses relatively.By the monochromatic CCD video cameras of Sony, with the image transfer of sample to Quantimet 520 MC iases (Leica, Cambridge UK).By Freehandhand-drawing figure around ice crystal, mark the crystal size of ice crystal.Each sample marks the size of at least 400 ice crystals.With the longest dimension of each crystal 2 D projection as being crystal size.Measure the number average crystal size of single crystal, as average mean crystal size.If the granularity of the crystal size in the time of 30-60 minute during to t=0 is similar or only have moderately that (less than 10%) increases, and/or crystal size is less than 20 microns, preferred 5-15 micron, and then expression has good ice crystallization inhibition again.

Embodiment 3

Standard Wei Keersi hardness test.

The Wei Keersi hardness test is an impression test, comprises that indentor with a pyramid type pushes the material surface and measures with the most advanced and sophisticated change in displacement of indentor and decide applied force.Measure power and displacement in impression load cycle and the unloading cycle.

This test is described in " plastics testing material handbook R.P.Brown volume, GeorgeGodwin Limited publication, The Builder Group, 1-3 Pemberton Row, Fleet Street, London, 1981.

Wei Keersi pyramid geometry is a kind of engineering industrial standard (BSi 427,1990).It is 136 ° that its most advanced and sophisticated place has a wedge angle.The following mensuration of hardness:

H wherein _VBe Wei Keersi hardness, F _MaximumBe that maximum, force (referring to Fig. 2) and the A that applies is the projected area of staying the impression on material surface.The geometry of supposing impression and formation the identical area A of measuring of geometry of indentor (being the Wei Keersi pyramid), therefore, can be according to the d among Fig. 2 _iThe depth of cup that provides is measured projected area.A＝24.5d _i ²

Embodiment 4

Contact gear ratio is measured

Use the microstructure image of ice confection to measure contact gear ratio, use low temperature scanning electron microscope method (SEM).Use " the ice river in Henan Province is insulted low temperature scanning electron microscope method research .I. technology and general microstructure " (A low temperature scanning electronmicroscopy study of ice cream. I. Techniques and generalmicrostructure) " food configuration " the 11st volume (1992), the technology of describing in the 1-9 page or leaf is carried out the image structure.

In the particulate complex, the contact gear ratio of particulate phase is defined as particle and particle contact-making surface (interface) the area ratio divided by total inside contact-making surface (interface) area.It is the measured value that particulate phase network forms degree.In ice confection, particle is to be positioned at intramatrical ice crystal, and therefore the contact gear ratio of ice is defined as:

C_{ii} = \frac{A_{ii}}{(A_{ii} + A_{im})}

C wherein _IiBe contact gear ratio, A _IiBe total contact-making surface (interface) surface area and the A of ice-ice contact-making surface (interface) _ImIt is contact-making surface (interface) surface area at ice-matrix contact-making surface (interface).Contact gear ratio can be measured according to the microstructure image on the arbitrary plane surface of cutting material.The Cryo-SEM image on the plane fracture surface of unaerated ice confection is enough to this.

By a winding displacement is placed on the microstructure image, calculates these lines and iced-ice and ice-the interception number of matrix contact-making surface (interface), and obtain contact gear ratio in conjunction with following equation:

C_{ii} = \frac{{2 N}_{ii}}{({2 N}_{ii} + N_{im})}

N wherein _IiThe number of=per unit length ice-ice interception, and N _ImThe number of=per unit length ice-matrix interception.

Ideally, total about 800 contact-making surfaces from 5 representative images of each sample structure.

For measuring contact gear ratio, each image is got two groups of measured values.One group of rule line is placed on after image goes up, calculates ice-matrix and ice-ice contact-making surface (interface), include only all tangible ice-ice contact-making surfaces (interface) by the interception number of these lines.Then, double counting, but comprise all possible ice-ice contact-making surface (interface) specifically.At this point, each image being carried out the maximum ice contact gear ratio measures and minimum ice contact gear ratio mensuration.Then, get these digital mean values as contact ratio.

Embodiment 5

Euler-Poincare assessment of indices

Use the microstructure image of ice confection to measure Euler-Poincare index, use low temperature scanning electron microscope method (SEM).Use " ice river in Henan Province icepro low temperature scanning electron microscope method research.I. technology and general microstructure " " food configuration " the 11st volume (1992), the technology imageization structure of describing among the pp1-9.

In the two-phase composite construction, can use the continuity degree of Euler-phase of Poincare assessment of indices.The Euler of phase-Poincare exponential quantity is low more, continuous more or coherent mutually in the microstructure.Euler-Poincare index can be positive number or negative.The definition of Euler-Poincare index visible " nothing of Euler-Poincare index estimate partially (Unbiased estimation of theEuler-Poincare characteristic " B. P. Pinnamaneni, C.Lantuejoul, J. P. Jernot and J. L. Chermant, Acta Sterlogica, 1989,8/2, p101-106).

For measuring the Euler-Poincare index of the ice in the ice confection, ias is discerned and used to ice on the microstructure image and matrix phase, use specific grapho-analysis program to measure ice phase Euler-Poincare index.Contrast in image will be iced automatically for ias and matrix distinguishing respectively when not enough, need the interface between the manual identification two-phase, can accurately measure Euler-Poincare index thus.

Can measure the Euler-Poincare index of the ice in the ice confection of producing by any processing approach.

Embodiment 6

Length-width ratio is measured

With sample in the Prolan environmental cabinet in about 12 hours of-18 ℃ of balances.By the ice confection thin layer being coated in thin glass sheet central authorities, preparation microscope micro slide.

Each micro slide is transferred on the microscope carrier of controlled temperature (18 ℃), collects the image (about 400 independent ice crystals) of ice crystal therein, and be sent to image storage and analytical system by video cameras.

Manually make the ice crystal image of depositing highlighted,, make whole crystal highlighted then by around it, marking circumference.Then, use to calculate and realize longest diameter (length), the shortest diameter (width), length-width ratio (length/width), measure highlighted crystal with the image analysis software of required calculating pixel number.

Calculate the mean aspect ratio of crystal.

Embodiment 7

Production has, and syrup ice cream sheet is stung in hollow " ring plate " formula moulding hard, crisp quality flatly.

By being prepared as follows syrup ice cream solution with following prescription:

% (weight)

Fructose 5.0

Carob gum 0.5

Citric acid 0.5

Flavouring agent/colouring agent 0.5

III type AFP ^*0.005

Add water to 100

^*Described in WO 97/02343

Total solid; 6.4%

-18 ℃ of following ice contents; 89.4wt%

Preparation syrup ice cream mixture

Use high shear mixer that all the syrup ice cream batchings except that AFP are mixed together about 3 minutes.The water that adds 80 ℃.After the mixing, the temperature of syrup ice cream mixture is about 55-65 ℃.

Add AFP then, and mix about 30 seconds with hot mixt.

Then, allow mixture carry out 81 ℃ pasteurize 25 seconds through heat-exchangers of the plate type.Then, mixture is cooled to about 4 ℃ before use in heat-exchangers of the plate type.

Preparation syrup ice cream product

Use Technohoy MF 75 scraper-type heat exchangers that syrup ice cream mixture half is freezing.Is that 15mm and internal diameter be the cylindrical spout of 11mm extrude by external diameter with syrup ice cream slush under approximately-2 ℃, forms long hollow tubular thing.Tube is hardened in-35 ℃ of airflow freezing machines, store down at-25 ℃ then.This hollow tubular thing is cut into about 1-2cmm length, form fritter (monobite) food.

The outer dia of fritter finished product is that about 20mm and syrup ice cream thickness are 2-3mm.

These goods are stable during making, pack, store and distributing.

Embodiment 8

The milk of chocolate flavouring is iced flat thin slice, and loosely is molded together and is wrapped in the chocolate.Provide goods new edible performance thus, it is easy and clean to operate.

By being prepared as follows milk ice (milk ice) pre-composition with following prescription:

% (weight)

Sucrose 13.2

42 DE corn syrup 2.8

Skimmed milk power 5.0

Full milk powder 11.2

Stabilizing agent 0.27

Emulsifying agent 0.2

Cocoa power 4.0

III type AFP ^*0.005

Add water to 100

^*Described in WO 97/02343

Total dissoluble solid; 35.3wt%

-18 ℃ of following ice contents; 52.1wt%

Use high shear mixer that all the milk ice batchings except that AFP are mixed together about 3 minutes.The water that adds 80 ℃.After the mixing, the temperature of milk ice mixture is about 55-65 ℃.

Add AFP then, and mix about 30 seconds with hot mixt.

Then, carry out 81 ℃ pasteurize 25 seconds with mixture homogeneous (2000psi) and through heat-exchangers of the plate type.Then, mixture is cooled to about 4 ℃ before use in heat-exchangers of the plate type.

Be coated on Gerstenberg and the Agger experimental scale drum-type refrigerator by the thin layer that about 0.5mm is thick, operate under the rotary speed of 5rpm, it is freezing that the chocolate milk is iced pre-composition.The area of drum surface is 0.2m ², it is cooled to-25 ℃ by circulation aqueous methanol cooling agent.After rotating cylinder is finished a rotation (about 12 seconds), the use sheet metal scrapes frozen coating and collects flat laminar milk ice from the surface.The independent flat thin slice that is produced is that 0.5-1mm is thick, 10-150mm is long and 1-10mm is wide.Then, use silicon paper flat thin slice loosely to be molded as the volume of grow up about 15cm and diameter 1-3cm.Then, the flat thin slice that this is molded is approximately-35 hardening in ℃ airflow freezing machine of operating down, then at-25 ℃ of storages.The flat rolls of sheets that this is molded is flooded or is soaked and hangs in the chocolate.

Embodiment 9-12

Preparation has the ice river in Henan Province of following prescription and insults composition:

Weight %

Sucrose 13.000

Skimmed milk power 10.000

Butter oil 8.000

Maltodextrin 40 4.000

Single palmitin (MGP) 0.300

Carob gum 0.144

Carrageenan L100 0.016

Flavouring agent 0.012

Add water to 100

Total dissoluble solid: 35wt%

-18 ℃ of following ice contents; 54wt%

Use high shear mixer that all ice rivers in Henan Province are insulted batching and be mixed together about 3 minutes.The water that adds 80 ℃.After the mixing, the temperature of syrup ice cream mixture is about 55-65 ℃.

After pasteurize, add III type AFP (as described in WO 97/02343) to the ice river in Henan Province by following concentration and insult in the pre-composition:

Embodiment 9-0.0005wt%

Embodiment 10-0.0025wt%

Embodiment 11-0.005wt%

Embodiment 12-0.001wt%

It is freezing to use Technohoy MF 75 scraper-type heat exchangers will ice river in Henan Province icepro pre-composition then, and the ice river in Henan Province is not introduced swell increment in insulting.To ice the river in Henan Province icepro extrudes under-4.3 to-4.6 ℃.Then goods are hardened in-35 ℃ of airflow freezing machines, store down at-25 ℃ then.

The four-point bending test that uses embodiment 1 to describe is measured apparent elastic modulus and bending (intensity).

The result compares with the control sample that does not contain AFP.The results are shown in Fig. 3 and 4, the embodiment that wherein contains AFP is represented by (◆) by () expression and the control sample that do not contain AFP.

Calculate Δ modulus, Δ modulus/original modulus, Δ intensity and Δ intensity/green strength.The results are shown in table 1.

The method of also using embodiment 3 to provide is measured Wei Keersi hardness.The results are shown in Fig. 5, the embodiment that wherein contains AFP is represented by (◆) by () expression and the control sample that do not contain AFP.

Calculate Δ H _V/ H _{V is original}With Δ H _V, the results are shown in table 1.

Table 1

Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	ΔH _V(MPa)	ΔH _V/H _{V is original}
Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	ΔH _V(MPa)	ΔH _V/H _{V is original}	9	7.3	1.7	0.2	0.5	1.65	6.2
10	104.8	2.46	0.3	0.67	1.25	9.02	9	7.3	1.7	0.2	0.5	1.65	6.2
10	104.8	2.46	0.3	0.67	1.25	9.02	11	208.3	4.9	0.8	1.76	2.7	10.2
12	109.6	2.58	0.37	0.822			11	208.3	4.9	0.8	1.76	2.7	10.2

The unaerated of embodiment 9-12 ice river in Henan Province insults to be used to provide does not have the discrete sheet of support, the flat thin slice that ring plate that provides as embodiment 7 and embodiment 8 provide.

Embodiment 13, Comparative Examples A-C

The ice river in Henan Province that has embodiment 10 prescriptions by embodiment 10 described preparations is insulted pre-composition, and it is described freezing with pre-composition to press embodiment 10 then, has the following swell increment (parts by volume (V of air _Air)):

Embodiment 13-does not have swell increment (0)

Comparative Examples A-43% swell increment (0.3)

Comparative example B-67% swell increment (0.4)

Comparative example C-100% swell increment (0.5)

The four-point bending test that uses embodiment 1 to describe is measured apparent elastic modulus and bending strength.

The result compares with the relevant control sample that does not contain AFP.The results are shown in Fig. 6 and 7, the embodiment that wherein contains AFP is represented by (◆) by () expression and the control sample that do not contain AFP.

Calculate Δ modulus, Δ modulus/original modulus, Δ intensity and Δ intensity/green strength.The results are shown in table 2.

The method of also using embodiment 3 to provide is measured Wei Keersi hardness.The results are shown in Fig. 8, the embodiment that wherein contains AFP is represented by (◆) by () expression and the control sample that do not contain AFP.

Calculate Δ H _V/ H _{V is original}With Δ H _V, the results are shown in table 2.

Table 2

Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	ΔH _V(MPa)	ΔH _V/H _{V is original}
Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	ΔH _V(MPa)	ΔH _V/H _{V is original}	13	132	5.1	0.5	2.3	1.25	8.9
A	40	4.7	0.1	1.5	0.2	4.0	13	132	5.1	0.5	2.3	1.25	8.9
A	40	4.7	0.1	1.5	0.2	4.0	B	17	3.3	0.05	1.1	0.15	4.3
C	6.6	1.6	0.02	0.4	0.05	2.1	B	17	3.3	0.05	1.1	0.15	4.3

The river in Henan Province icepro is iced in the unaerated of embodiment 13 can be used for making nothing support discrete sheet, as the ring plate of embodiment 7 descriptions and the flat thin slice of embodiment 8 descriptions.Yet, use the nothing support discrete sheet of the ice river in Henan Province icepro manufacturing of Comparative Examples A-C self not support and to subside at storage with during distributing.

Embodiment 14-17

By being prepared as follows syrup ice cream solution with following composition:

Weight %

Sucrose 20.0

Carob gum 0.2

Add water to 100

Total dissoluble solid; 20.2wt%

-18 ℃ of following ice contents; 70wt%

Be prepared as follows syrup ice cream solution:

After pasteurize, III type AFP (as described in WO 97/02343) is added in the syrup ice cream solution by following concentration:

Embodiment 14-0.0005%

Embodiment 15-0.0011%-

Embodiment 16-0.0025%

Embodiment 17-0.005%

Syrup ice cream solution is freezing in Technohoy MF 75 scraper-type heat exchangers, do not introduce swell increment.The syrup ice cream is extruded under-3.9 to-5.6 ℃.Then goods are hardened in-35 ℃ of airflow freezing machines, store down at-25 ℃ then.

The result compares with the control sample that does not contain AFP.The results are shown in Fig. 9 and 10, the embodiment that wherein contains AFP is represented by (◆) by () expression and the control sample that do not contain AFP.

Calculate Δ modulus, Δ modulus/original modulus, Δ intensity and Δ intensity/green strength.The results are shown in table 3.

The method of also using embodiment 3 to provide is measured Wei Keersi hardness.The results are shown in Figure 11, the embodiment that wherein contains AFP is represented by (◆) by () expression and the control sample that do not contain AFP.

Calculate Δ H _V/ H _{V is original}With Δ H _V, the results are shown in table 3.

Table 3

Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	ΔH _V(MPa)	ΔH _V/H _{V opens up the beginning}
Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	ΔH _V(MPa)	ΔH _V/H _{V opens up the beginning}	14	243	1.14	0.3	0.8	3.8	1.12
15	471	2.2	0.6	1.5	3.2	0.9	14	243	1.14	0.3	0.8	3.8	1.12
15	471	2.2	0.6	1.5	3.2	0.9	16	662	3.1	0.7	1.7	4.0	1.2
17	785	3.7	1.2	3.0	7.0	2.0	16	662	3.1	0.7	1.7	4.0	1.2

The syrup ice cream composition of embodiment 14-17 can be used for making does not have the discrete sheet of support, as the ring plate of embodiment 7 descriptions and the flat thin slice of embodiment 8 descriptions.

Embodiment 18-21

The syrup ice cream solution that has following composition by embodiment 14-17 preparation:

Weight %

Sucrose 20.0

Carob gum 0.2

Add water to 100

Total dissoluble solid; 20.2wt%

-18 ℃ of following ice contents; 70wt%

After pasteurize, add III type AFP (as described in WO 97/02343) to syrup ice cream solution by following concentration:

Embodiment 18-0.0005%

Embodiment 19-0.0011%

Embodiment 20-0.0025%

Embodiment 21-0.005%

Then, syrup ice cream solution is static freezing.The metal die of splitting that the impouring of syrup ice cream solution is used for manufacturing machine test block (referring to embodiment 1).Then their static freezing refrigerations under-25 ℃ are spent the night.

Next day,, put into Polythene Bag and refrigerate that day before carrying out mechanical test down at-25 ℃ with the prod demoulding.

The result compares with the control sample that does not contain AFP.The results are shown in Figure 12 and 13, the embodiment that wherein contains AFP is represented by (◆) by () expression and the control sample that do not contain AFP.

Calculate Δ modulus, Δ modulus/original modulus, Δ intensity and Δ intensity/green strength.The results are shown in table 4.

Table 4

Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}
Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	18	871	2.7	0.85	2.7
19	985	3.1	0.96	3.0	18	871	2.7	0.85	2.7
19	985	3.1	0.96	3.0	20	1269	4.0	1.4	4.2
21	1347	4.2	1.5	4.8	20	1269	4.0	1.4	4.2

Embodiment 22 and 23, comparative example D

Weight %

Sucrose 13.000

Skimmed milk power 10.000

Butter oil 8.000

Maltodextrin 40 4.000

MGP 0.300

Carob gum 0.144

Carrageenan L100 0.016

Flavouring agent 0.012

Add water to 100

Total dissoluble solid; 35wt%

-18 ℃ of following ice contents; 54wt%

Use high shear mixer that all ice rivers in Henan Province are insulted batching and be mixed together about 3 minutes.The water that adds 80 ℃.After the mixing, the temperature of syrup ice cream mixture is about 55-65 ℃.Then, carry out 81 ℃ pasteurize 25 seconds with mixture homogeneous (2000psi) and through heat-exchangers of the plate type.Then, mixture is cooled to about 4 ℃ before use in heat-exchangers of the plate type.

Embodiment 22-0.0005wt%

Embodiment 23-0.005wt%

Comparative example D-does not contain AFP

Then, it is freezing to use Technohoy MF 75 scraper-type heat exchangers will ice river in Henan Province icepro pre-composition, and the ice river in Henan Province is not introduced swell increment in insulting.To ice the river in Henan Province icepro extrudes under-4.4 to-5.4 ℃.Then, goods are hardened in-35 ℃ of airflow freezing machines, store down at-25 ℃ then.

Press embodiment 4 and measure contact gear ratio.

The results are shown in table 5.

Table 5

Embodiment	Contact gear ratio
Embodiment	Contact gear ratio	22	0.2
23	0.3	22	0.2
23	0.3	D	0.1

Embodiment 24 and 25, comparative example E

Weight %

Sucrose 20.0

Carob gum 0.2

Add water to 100

Total dissoluble solid; 20.2wt%

-18 ℃ of following ice contents; 70wt%

Press embodiment 12 preparation syrup ice cream solution.

Embodiment 24-0.0005wt%

Embodiment 25-0.005wt%

Comparative example E-does not contain AFP

Then, use Technohoy MF 75 scraper-type heat exchangers that syrup ice cream solution is freezing, do not introduce swell increment.The syrup ice cream is extruded under-3.9 to-5.6 ℃.Then, goods are hardened in-35 ℃ of airflow freezing machines, store down at-25 ℃ then.

Press embodiment 4 and measure contact gear ratio.The results are shown in table 6.

Table 6

Embodiment	Contact gear ratio
Embodiment	Contact gear ratio	24	0.24
25	0.22	24	0.24
25	0.22	E	0.11

Embodiment 26, comparative example F

Weight %

Sucrose 13.000

Skimmed milk power 10.000

Butter oil 8.000

Maltodextrin 40 4.000

MGP 0.300

Carob gum 0.144

Carrageenan L100 0.016

Flavouring agent 0.012

Add water to 100

Total dissoluble solid; 35wt%

-18 ℃ of following ice contents.

Embodiment 26-0.005wt%

Comparative example F-does not contain AFP

Press embodiment 5 and measure Euler-Poincare index.

The results are shown in table 7.

Table 7

Embodiment	Euler-Poincare index (mm ^-2)
Embodiment	Euler-Poincare index (mm ^-2)	26	-577
F	339	26	-577

Embodiment 27, comparative example G

Weight %

Sucrose 20.0

Carob gum 0.2

Add water to 100

Total dissoluble solid; 20.2wt%

-18 ℃ of following ice contents; 70wt%

Press embodiment 12 preparation syrup ice cream solution.

After pasteurize, III type AFP (described in WO 97/02343) is added in the syrup ice cream solution by following concentration:

Embodiment 27-0.005wt%

Comparative example G-does not contain AFP

It is described to press embodiment 21, and syrup ice cream solution is static freezing, does not introduce swell increment.

Press embodiment 5 and measure Euler-Poincare index.

The results are shown in table 8.

Table 8

Embodiment	Euler-Poincare index (mm ^-2)
Embodiment	Euler-Poincare index (mm ^-2)	27	-383
G	4.3	27	-383

Embodiment 28

By being prepared as follows milk ice solution with following composition:

％ (w/w)

Sucrose 13.2

Corn syrup 2.8

Full milk powder 11.2

Skimmed milk power 5.0

Stabilizing agent 0.27

Emulsifying agent 0.20

Colouring agent/flavouring agent 0.06

AFP ^* 0.005

Add water to 100

^*Described in WO 97/02343

Add III type AFP (described in WO 97/02343) then in two, and to wherein half with mixture.

Then, will suckle ice solution static freezing.The ice solution impouring of will suckling is used for the distinguish metal die of manufacturing machine test block (referring to embodiment 1).Then their refrigeration is spent the night, with static freezing down at-25 ℃.Next day,, put into Polythene Bag and refrigerate that day before carrying out mechanical test down at-25 ℃ with the prod demoulding.

The milk ice result that will contain AFP compares with the control sample that does not contain AFP.

Calculate Δ modulus, Δ modulus/original modulus, Δ intensity and Δ intensity/green strength.The results are shown in table 9.

Table 9

Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}
Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	28	756	16.2	1.81	6.68

Embodiment 29

Be prepared as follows milk ice solution with following composition:

％(w/w)

Sucrose 13.2

Corn syrup 2.8

Full milk powder 11.2

Skimmed milk power 5.0

Stabilizing agent 0.27

Emulsifying agent 0.20

Colouring agent/flavouring agent 0.06

AFP ^* 0.005

Add water to 100

^*Described in WO 97/02343

The ice solution of will suckling is freezing in Technohoy MF 75 scraper-type heat exchangers, does not introduce swell increment.The syrup ice cream is extruded under-3.9 to-5.6 ℃.Then, goods are hardened in-35 ℃ of airflow freezing machines, store down at-25 ℃ then.

Calculate Δ modulus, Δ modulus/original modulus, Δ intensity and Δ intensity/green strength.The results are shown in table 10.

Table 10

Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}
Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	29	290	5.08	0.968	4.17

Embodiment 30

Press the contents production hollow ring plate type fritter syrup ice cream sheet of embodiment 7.

Production contains and does not contain the different sugar water-ice cake sheet of III type AFP.The ring plate that does not contain III type AFP does not have crisp quality, and makes it easily to be out of shape and to break with hand.

It is online that every kind sample is placed on stainless steel sift, and this screen cloth is in the temperature controlled environment (temperature=+ 24 ℃).Working sample is to the loss in weight of time, because sample melts and pass through the screen cloth drip in time.Measure the mean value of 3 repeated tests of two kinds of samples that need research.The results are shown in table 11.

Table 11

Time	Wt loss is in the same old way	Wt loss+AFP	Mass loss is in the same old way	Mass loss+AFP
Time	Wt loss is in the same old way	Wt loss+AFP	Mass loss is in the same old way	Mass loss+AFP	(minute)	(％)	(％)	(g)	(g)
4	0.4	0.0	0.06	0.00	(minute)	(％)	(％)	(g)	(g)
4	0.4	0.0	0.06	0.00	5	4.4	0.0	0.60	0.00
6	7.0	0.0	0.96	0.00	5	4.4	0.0	0.60	0.00
6	7.0	0.0	0.96	0.00	7	9.2	0.0	1.26	0.00
8	10.2	0.0	1.40	0.00	7	9.2	0.0	1.26	0.00
8	10.2	0.0	1.40	0.00	9	10.6	0.0	1.45	0.00
10	10.8	0.0	1.48	0.00	9	10.6	0.0	1.45	0.00
10	10.8	0.0	1.48	0.00	11	11.6	0.4	1.59	0.05
12	13.0	1.4	1.79	0.19	11	11.6	0.4	1.59	0.05
12	13.0	1.4	1.79	0.19	13	14.1	4.0	1.94	0.54
14	16.0	6.2	2.19	0.85	13	14.1	4.0	1.94	0.54
14	16.0	6.2	2.19	0.85	15	17.1	10.8	2.35	1.48

From data as can be seen, to being different with the melting of AFP goods in the same old way.After 4 minutes, see for first of the contrast goods, need be and contain the AFP goods greater than 10 minutes.Goods are almost very fast just begins to lose its structural intergrity in contrast, melt up to it and contain the hollow and annular that the goods of AFP are kept perfectly.

Embodiment 31

The assay method of ice sheet mechanical performance.

Use three point bending test to measure mechanical performance.

Can use three point bending test to measure many mechanical performances of ice confection material.The mechanical performance of measuring is Young's modulus (apparent) and bending strength.

In bend test, make test block distortion, measure the power that applies and the deflection of test block simultaneously.The n-lustrative data group of ice confection is shown among Fig. 1.The slope that begins straight line portion according to this curve is measured apparent elastic modulus.

3-point bend test need be produced the parallel edges sq.rd of ice confection material.This can obtain by any suitable means.

In this specific application, use silicon rubber mould to make the parallel edges sq.rd of ice confection, produce and be of a size of the rectangular of 70 * 10 * 2mm.

Mixture slightly overfill is filled up mould and controlled temperature plate (being decided to be-30 ℃) be lowered on the mould, with the full whole width of toilet cover, and thorough freezing.Then, sample-20 ℃ of following balances, is cut into 50mm length afterwards.Then, the ice confection balance that this 50mm is long is spent the night to-18 ℃, carries out following analysis afterwards.

Test method is described in " biomethanics material, a kind of hands-on approach " J.F.V.Vincent and compiles, and IRL Press publishes, the Oxford University Press, and Walton Street, the Oxford is in 1992.Test comprises each club is placed on 2 carriers, and makes it crooked, and the central authorities that make the club upper surface until being exerted pressure by the 3rd carrier produce fracture.Crooked applied force of record and the mobile displacement that contacts in entire test.The decrease speed of mobile vehicle is per minute 10mm.

Provide the apparent elastic modulus of material by following equation:

In these tests, span (S) is 30mm.

Embodiment 32

Preparation has the syrup ice cream solution of following composition:

％w/w

Sucrose 5

Carob gum 0.2

AFP ^* 0.005

Add water to 100

^*Described in WO 97/02343

Total dissoluble solid; 5wt%

-18 ℃ of following ice contents; 92wt%

Be prepared as follows syrup ice cream solution:

Mixture is cooled to about 4 ℃ in brine bath.

After the cooling, III type AFP (described in WO 97/02343) is added in the syrup ice cream solution.

Press the thin syrup ice cream layer of content manufacturing of embodiment 31, use embodiment 31 described test determination apparent elastic modulus and bending strengths then.

The result compares with the control sample that does not contain AFP.

Calculate Δ modulus, Δ modulus/original modulus, Δ intensity and Δ intensity/green strength.The results are shown in table 12.

Table 12

Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}
Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	32	1224	1.6	2.3	1.6

Embodiment 33

Repeat embodiment 32, difference is the syrup ice cream solution that is prepared as follows:

％w/w

Sucrose 20

LBG 0.2

AFP ^* 0.005

Add water to 100

^*Described in WO 97/02343

Total dissoluble solid; 20.2wt%

-18 ℃ of following ice content: 70wt%

The results are shown in table 13

Table 13

Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}
Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	33	1121	5.2	2.2	2.8

Embodiment 34

The syrup ice cream solution that has following composition by embodiment 17 preparations:

％w/w

Sucrose 10.0

Glucose 5.0

LBG 0.2

Citric acid 0.5

AFP ^* 0.005

Colouring agent/flavouring agent 0.2

Add water to 100

^*Described in WO 97/02343

According to the thin syrup ice cream layer of content preparation of embodiment 31 and test determination apparent elastic modulus and the bending strength of using embodiment 31 to describe.

The result compares with the control sample that does not contain AFP.

Calculate Δ modulus, Δ modulus/original modulus, Δ intensity and Δ intensity/green strength.The results are shown in table 14.

Table 14

Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}
Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	34	1936	3.3	3.1	6.9

Embodiment 35

Repeat embodiment 34, difference is to use the milk icing compositions with following prescription:

％w/w

Fructose 5.0

LBG 0.5

Citric acid 0.5

Colouring agent/flavouring agent 0.2

AFP ^* 0.005

Add water to 100

^*Described in WO 97/02343

The results are shown in table 15.

Table 15

Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}
Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	35	111	1.4	0.6	0.95

Embodiment 36

Weight %

Sucrose 13.500

Defatted milk concentrate (30% solid content) 24.000

Rare cream (40% fat) 43.000

Yolk (not dulcification) 4.500

Vanilla flavor 1.000

Add water to 100

Total dissoluble solid; 45wt%

-18 ℃ of following ice contents; 46wt%

Use high shear mixer that all ice rivers in Henan Province are insulted batching and be mixed together about 3 minutes.The water that adds 80 ℃.After the mixing, the temperature that the ice river in Henan Province is insulted mixture is about 38-45 ℃.

After pasteurize, add I type AFP (from AF Protein) to the ice river in Henan Province by following concentration and insult in the pre-composition:

Embodiment 36-0.001wt%

Then, it is freezing to use Technohoy MF 75 scraper-type heat exchangers will ice river in Henan Province icepro pre-composition, does not introduce swell increment.To ice the river in Henan Province icepro extrudes under-4.8 to-5.5 ℃.Then goods are hardened in-35 ℃ of airflow freezing machines, store down at-25 ℃ then.

The result compares with the relevant control sample that does not contain AFP.

Calculate Δ modulus, Δ modulus/original modulus, Δ intensity and Δ intensity/green strength.

The results are shown in table 16.

Table 16

Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}
Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	36	138	4.2	0.408	1.09

Embodiment 37

wt％

Sucrose 18

Carob gum 0.18

Hydrolysis milk proem (Hyfoama DS ^*) 0.1

Grass AFP solution ^*30.0

Add water to 100

^*As described in WO 98/04699.The use amount of grass (grass) AFP solution suppresses needed minimum according to the crystallization again that embodiment 2 definition are provided and decides.

^*Hyfoama DS is the trade mark of Quest International.

Total dissoluble solid; 18wt%

-18 ℃ of following ice contents; 73wt%

Make the control mixture do not contain AFP, replace careless AFP solution with the water of 30wt%.

Then, mixture is carried out 81 ℃ pasteurize 25 seconds through heat-exchangers of the plate type.Then, mixture is cooled to about 4 ℃ before use in heat-exchangers of the plate type.

Add AFP after the pasteurize.

Syrup ice cream solution is freezing in Technohoy MF 75 scraper-type heat exchangers, do not introduce swell increment.The syrup ice cream is extruded under-2.6 to-3.6 ℃.Then goods are hardened in-35 ℃ of airflow freezing machines, store down at-25 ℃ then.

The result compares with the control sample that does not contain AFP.

Calculate Δ modulus, Δ modulus/original modulus, Δ intensity and Δ intensity/green strength.The results are shown in table 17.

Table 17

Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}
Embodiment	ΔE(MPa)	ΔE/E _Original	Δσ _u(MPa)	Δσ _u/σ _{U is original}	37	230	0.84	0.615	1.03

Embodiment 38

wt％

Sucrose 18

Carob gum 0.18

Hydrolysis milk proem (Hyfoama DS ^*) 0.1

Grass AFP solution ^*30.0

Add water to 100

^*As described in WO 98/04699.The use amount of grass AFP solution suppresses needed minimum according to the crystallization again that embodiment 2 definition are provided and decides.

^*Hyfoama DS is the trade mark of Quest International.

Total dissoluble solid; 18wt%

-18 ℃ of following ice contents; 73wt%

After the pasteurize AFP solution is added in the syrup ice cream solution.

Then that syrup ice cream solution is static freezing.The metal die of splitting that the impouring of syrup ice cream solution is used for manufacturing machine test block (referring to embodiment 1).Then their refrigeration is spent the night, with static freezing down at-25 ℃.Next day,, put into Polythene Bag and refrigerate that day before carrying out mechanical test down at-25 ℃ with the prod demoulding.

The four-point bending test that uses embodiment 1 to describe is measured apparent elastic modulus.

The result compares with the control sample that does not contain AFP.

Calculate Δ modulus, Δ modulus/original modulus.The results are shown in table 18.

Table 18

Embodiment	ΔE(MPa)	ΔE/E _Original
Embodiment	ΔE(MPa)	ΔE/E _Original	38	146	2.59

Claims

1. a thin nothing supports the ice confection of discrete patch form, and it is stable at packing, storage and selling period, and the swell increment of this ice confection is less than 10%, and wherein ice confection contains antifreeze protein and has following mechanical performance:

Δ modulus/original modulus 〉=0.4, and/or

Δ intensity/green strength 〉=0.4; Precondition is to work as

Δ modulus/original modulus≤6.0 o'clock,

Δ modulus 〉=50MPa, and/or when Δ intensity/green strength≤2.0,

Δ intensity 〉=0.2MPa.

2. the ice confection of claim 1, Δ modulus/original modulus 〉=0.4 wherein, precondition is when Δ modulus/original modulus≤0.6, Δ modulus 〉=70MPa.

3. the ice confection of claim 2, wherein Δ modulus 〉=90MPa.

4. the ice confection of claim 3, wherein Δ modulus 〉=100MPa.

5. the ice confection of claim 1, Δ modulus/original modulus 〉=1.0 wherein, precondition is when Δ modulus/original modulus≤6.0, Δ modulus 〉=100MPa.

6. the ice confection of claim 5, wherein Δ modulus 〉=200MPa.

7. the ice confection of claim 1, wherein Δ intensity/green strength 〉=0.7.

8. the ice confection of claim 7, wherein Δ intensity/green strength 〉=1.5.

9. the ice confection of claim 1, wherein Wei Keersi hardness measurement Δ H _V/ H _{V is original}〉=0.3, precondition is as Δ H _V/ H _{V is original}≤ 5.0 o'clock, Δ H _V〉=0.3.

10. the ice confection of claim 1, its contact gear ratio at least 0.2 and when its ice content when measuring down for-18 ℃ be 50-90wt%.

11. the ice confection of claim 1, its Euler-Poincare index are less than-150mm ^-2And when its ice content when measuring down for-18 ℃ is 50-90wt%.

12. the ice confection of claim 1, wherein ice confection is selected from syrup ice cream and milk ice.

13. each described ice confection of claim 1-12 wherein selects antifreeze protein so that it that the length-width ratio of ice crystal is reached greater than 1.9.

14. each described ice confection of claim 1-12, wherein antifreeze protein is an AFPIII type HPLC-12 albumen.

15. each described ice confection of claim 1-12, wherein the thickness of sheet is 0.5-5mm.

16. each described ice confection of claim 1-12, wherein the ice content of ice confection is when be at least 30% volume when measuring down for-18 ℃.

17. the ice confection of claim 16, wherein ice content is when be at least 40% volume when measuring down for-18 ℃.

18. the ice confection of claim 17, wherein ice content is when be at least 50% volume when measuring down for-18 ℃.

19. each described ice confection of claim 1-12, wherein the total dissoluble solid content of ice confection is less than 40wt%.

20. the ice confection of claim 19, wherein the total dissoluble solid content of ice confection is less than 25wt%.

21. the ice confection of claim 20, wherein the total dissoluble solid content of ice confection is less than 15wt%.

22. the purposes of each described ice confection of claim 1-12 in the ice confection goods that provide the stable thin nothing of packing, storage and selling period to support the discrete patch form.